Process of making and recovering ammonia, &amp;c.



W. J. DUNNAGHIE. PROCESS 0F MAKING AND RECOVERING AMMONIA, &o. APPLIUATION FILED APn.s,1,9o.

2 SHEBTS-SHBETJ.

Patented Dec. 14, 1909.

W.' J. DUNNACHIE. PROCESS OP MAKING AND REOOVRING AMMONIA, dao.

APPLIOA'LION FILED APB. 3, 1908.

Patented Dec. 14, 1909..

UNITED srirrns rafrnnr orrion.

WILLIAM JAMES DUNNACHIE, or oofirnnrnen, scorLAnD.-

PROCESS OF MAKING AND RECOVERING A MIVIDNIA, &c.

Specification of Letters Patent. Patented Dec. '14, 1909.

'Application filed April 3, 1908. Serial No. 425,079.

To all whom it may con/cem:

Be it known that I, WILLIAM JAMES DUN- Niioiiin, of Vievvield, Coatbridge, in the county of Lanark, Scotland, have invented a certain new and useful Process of Making and Recovering Ammonia. and other By- AProducts, of which the following is a specification.

This invention relates to blast or other furnaces, gas-producers,v retorts, coke-ovens and the like, 1n which coke, coal, or other charge, has been so treated, but not so'that lo I from cokevor anthracite fed' furnaces, gasproducers, andthe like, because the amount .of recoverablel residuals in the 'gas is s osmall, under present conditions, that their profitable extraction is impossible.

The object of my invent-ion is to convert Whatmay be termed the fixed nitrogen of the coal, coke, shale, or other carbo-nitrogenous matter, cyan'ogen and its compounds, and in -cases Where air is introduced, possibly some of the nitrogen of the blast or air, into .ammonia and thereby largely to in- 'crease the present yield of ammonia from such sources, and to bring anthracite and cokefedfurnaces and the like into the cat-egory of profitable producers of ammonia. To accomplish-.this object, I Withdraw a ortion of the hotter gas, in the case of the 'last-furnace and other force-blast furnaces from above the tvvyers, and, in the case of coke-ovens, retorts and the like, Where air is not introduced, from the hotter regions,

`I cause this gas immediately after its Withdrawal and before its temperature has been greatly reduced, .to Vmix intimately With steam, Water-spray and in certain contingencies, a small' volume of air and thereafter 'to' pass through Water, in an external vessel,'as will be hereinafter described.

In order that my invention maybe 'prop-A erly understood and readily carried into effect, I have hereunto appended tivo sheets of drawings, of Which- 4 1 -Figure 1 illustrates in vertical sectiona ,2, all hereinafter more fully referred described.

blast furnace .to which thel improvements embodying my invention are applied.v Fig. 2 is a vertical section of a mixing vessellor apparatus designed to be used in connection with the blast furnaceillustrated in Fig.`1.

Fig. 3 is a section of a modified forni' of the loiver part of the mixing vessel or appa' ratus, shown in Fig. 2, drawn to enlarged K scale and constructed With a brickbrdge or arch. Fig. 4 is an end elevation ofA a inodification of the mixing vessel or apparatus illustrated in Fig. 2. Fig. 5 is a side elevation of the'inopliticat-ion shown in Fig. 4. Fig. 6 is an elevation of the plant embody` ing the apparatus, illustrated in F igs.y 1 and to' and Referring first to Figs. l and 2 of the drawings, which show one embodiment of a portion of the device for lcarrying out myv improved process, the blast furnaceV 1 is provided below with the usualv horseshoe air-blast main Zyconnecting'by downwardly projecting ducts 3 with the twyers 4 com? municating With the interior of the furnace immediatelyabove the crucible 5. In the.

upper end of the furnace, the bell 6 is adapted to admit the' charge in the usual manner from the hopper 7. In the hotter openings 8 (see Fig. l) are provided' into the interior of the furnace 9.

V yregions above the tWyers 4, one or' more Into' these openings I insert brick-lined .tubes 10, connecting at their outer extremities with a brick-lined liorseshoe main 11, for thereception of the escaping gas from the hotter regions of the blast-furnace. 'From the horse-shoe main l1, a brick-lined iron tube l2 connects With what I` have termed the mixer, 13, (Figs. 2 and 4). The "mixer 13 (Fig. 2) is a brick-liiied chamber filled with brick-checker-Work'14, or other suitable' intersticed material, the object of .which is to insure the intimate mixture ofjthev hotgas with steam or Waterspiay, or: mixtureA of steam and Water and, when required, asmall volume of air, for thepurpose of converting f thevcyanids into ammonia. Water-spray or the mixture of botli,ve1`iterfby The steam or the pipes l5 which are perforated byV a series of holes sov as more effectually to secure this They are arranged 'to 4bring .the steam or Water-spray into contact With the liot gas immediately on its en#V intimate mixture.

trance into the mixer and before"itfha's` greatly cooled. 'When required, av smallvolunie of compressed air-is blown in by the.

horizontal pipe 16 perforated 4 on its upper side.

The rush of air produces a further spray of water while the escaping air inthe of the cyanids into ammonia'and prevents the formation of carbonio acid as a constituent of thev escaping gas. The distribution of the steam and Waterlspray may be attained in many other ways. According to onemode of operation, the gas and ammonia are conveyed from themixer by a suitable pipe-17 -to the green-gas tube 33, for conveyance to the recovery Works, when there are such; or according to another method of procedure, the' gas and ammonia are conducted from the mixer 13 through the pipe 29 into the horse-shoe main from whence it is admitted into the upper cooler portions of the furnace to'be'treated preliminary to its conveyancev to the ammonia-recovery works.

' The alkalies contained in the gas are rel point.

' tained ,in solutionaiii the mixer 13, where '25 I i they are gradually concentrated and periodically drawn oft' by the pipe 18, into the receiver 19, and thence by compressed air, operating through the pipe 20, the partially concentrated alkaline solution may be discharged into the concentrator 21', for fur- .ther concentration by the heat Vemanating from the mixer 13. The ammonia, distilled olf during this further concentration, passes into the tube 17; 1??

In Fig. 3 the gas entering the mixer I13 is vintercepted by a brick bridge or ar'chf22,

.which 'dips into the water contained in thc lower body of the mixer. The gas is brought into contact with steam, air, and waterspray which enter the mixer bythe pipes 15, and is then forced or drawn under the arch By another modification,` see Figs. 4 and 5, l cause the hot gas to pass into the mixer 13, which is an iron vessel, (brick-lined where necessary) partially filled with water to the level 23, and subdivided as to its length by a series of serrated baille iron or steel plates 24 which dip into the water several inches. The hot gas on entering the mixer is intimately mixed with steam, air and water-spray and-is forced or drawn under the baliie plates whereby -it is divided into fine streams bythe serrated edges 25, and thereby brought into intimate contact with the water "which, by the heat communicated `from the gas, is soon raised to boiling The net result of the violent ebullition of,`and r'ushof 'gas and air through the water, will be the'automatic creation of an atmosphere of steam, water-spray and gas, which is the condition most favorable to the complete conversion of the cyanids into ammonia, The amount of injected steam is, by thismeans, reduced to a minimum. The

evaporation ofthe'water is made good by the admission of water to a sufficient amount.

The gas and ammonia pass oil" by the tube 17, into the green-gas main for treatment at the ammonia recovery Works; but ,Where such do not exist, they may be led into one or more saturators '37, see Fig. 6, containing lsulfuric acid where the ammonia Will be immediately converted into sulfate of am; mo'ma and vthe escaping gas conveyed by suitable pipes to condensers for distribution as required; and the water from the 0011-' concentrate may be subsequently filtered and evaporated to dryness for disposal or reintroduction with or without additions to the furnace' charges. Again, said concentrate may be conveyed directly to the receiver 19 v from which it is piped to the recovery works for the extraction of the ammonia, potash and soda contained in it. Any deposit vcollecting in the interior of lthe receivers 19 (Figs. 2, 4 and 5) may be removed through,

the clearing door 28.

Whenever the volume of gasto be treated is large and at a high temperature, itis desirable to pass it successively through both heat sustained by. the furnace, may be made good by introducing an excess of combustible in the charge or'by introducing super- `mixers shown in Figs. 2 and -3. The loss of heated gas above the level at which the gas is drawn off.

By means of a third modification, the gas and steam after treatment with sulfuric acid, may be conveyed by a suitable tube 29 (Fig. 6) to a second horse-shoe main 30 l (Figs. 1 and G) communicating by one or vmore twyers 31 with the upper regions of the interior of the furnace 9. From the main 30, the gas and steanrare introduced to the furnace,.wliere they react upon the into ammonia by means of the steam conveyed With the gas. The steamv on entering this cooler region or zone of the furnace, is in part, decomposed b the red hot carbon nascent state, will immediately combine with some of the fixed nitrogen of the raw material or with cyanogen gas,` (if present) to xed nitrogen of the fuel for its conversion, f

whereby 'hydrogen is liberated which, in its form ammonia. This ammonia will be prtected` from decomposition, in its passage through the hot raw material to the main gas tube 33, by the excess of steam, free hyvided with liot or cold blast.

' ash.

drogen and hydrocarbon gases contained in the. mixed gas. The yield of ammonia will thus be greatly increased, irrespective of Whether the raw material used be coal, coke, anthacite, or other carbo-nitrogenous materia I will now explain my invention as ap lied' to the extract-ion of valuable products rom waste heaps of carbo-nitrogenous matter, such as are found at most collieries, and shale mines; lalso the applicat-ion of m'y rocess to the economic manufacture of gas for metallurgical and other purposes from such Waste heaps, round and small coal, lignite, peat, or other form of such carbonitrogenous material. As applied to such purpose, I erect one or more blastfurnaces prolf desired, the fuel charged into the furnace or furnaces through the bell and hopper may be mixed with the necessary proportions of lime or other flux to form a liquid slag with the The hot gas is extracted and treated in the manner already described. Steam fromtthe horse-shoe main (see Fig. l) is injected through the twyers 31, and the gas escaping from the 'tub 32, combined with that from the mixer 1S, is conveyed bythe tube 33, to a suitable tar and ammonia 'rccovery plant, whence the purified gas is 'distributed to the metallurgical works, for heating-stoves, boilers, gas-enginesand the like; By a careful mixture of the materials charged into these gas producers, a slag can lbe produced of a composition admirably suited for the manufacture of cement.

It is obvious from the nature of my iinproved process that it is one that accommodates itself to many modifications of the plant l have shown for carrying it out.

i l claim:-

1. The processof recovering ammonia and other byeproducts which consists in taking ofi', at the hotter regions, the hot gases from blast furnaces, gas producers and similar appliances consuming a mixture of carbo-nitrogeiious fuel, in treating these hot gases immediately after 'removal from the furnace 'with an aqueous fluid and thereafterwith sulfuric acid; in 4introducing them againto the cooler part of the furnace at a point above the level from which they were drawn;

vin collecting the converted gas from the top of the'furnace; and finally in absorbing the ammonia therefrom.

2. The method of recovering. ammonia and other lay-products from carbo-nitrogenous substances which consists in taking off, at the hotter regions, a portion of the furnace gases from blast-furnaces, gas-producers and similar appliances consuming carbo-nitrogenous fuel, in treating said gases with an aqueous fluid immediately after removal from the furnace, and thereafter with sulfuric acid; and finally reintroducing the gases into the cooler and upper region of the furnace.

3. The process for the recovery of animonia which consists in drawing olf, at the hotter regions, a portion of the gases from blast-furnaces, gas producers and similar appliances consuming a mixture of carbo-nitrogenous fuel, in treating said portion with an aqueous fluid immediately after removal from the furnace, to convert the cyanide into ammonia and thereafter with sulfuric acid to absorb said ammonia; in reiutroducing the gases so treated into the upper and cooler region of the furnace and nally iii collect ing the gases from the top of the furnace.

4l. rlhe process for the manufacture of ammonia which consists in taking cyanogencontaining gas from the hotter regions of blast-furnaces, gas-producers and similar ap pliances consuming carbo-nitrogenous fuel, in treating the same with an aqueous fluid in the presence of an intermittent blast of air to convert the cyanid into ammonia; and in absorbing the ammonia.

5. The process of recovering ammonia from the gases of blastfuriiaces, gas-producers and similar appliances, consuming carbo-nitrogenous fuel, which process consists in drawing off, at the hotter regions, portions of the hot gases; in submitting such gases immediately after removal from the furnace to the action of an aqueous fluid in the presence of an intermittent blast of air; in recovering the fixed allralies formed by such action; and finally in absorbing the am monia.l l

In witness whereof I have hereunto set my hand in the presence of two witnesses.

WILLIAM JMES' DUNNACIIIE. lYitnesses JOHN Linnmi, JOHN l". LIDDLE. 

